Acetyl chloride → HCID 136348417, compound

HRID 1748717Notes

Reaction equation

HRID 1748717 reaction equation
C([Cl:4])(=O)C.[CH3:5][N:6]1[C:10]2[NH:11][CH2:12][CH2:13][S:14][CH:15]([CH:16]3[CH2:21][CH2:20][N:19](C(OC(C)(C)C)=O)[CH2:18][CH2:17]3)[C:9]=2[C:8]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][N:30]=2)=[N:7]1>CO>[ClH:4].[ClH:4].[CH3:5][N:6]1[C:10]2[NH:11][CH2:12][CH2:13][S:14][CH:15]([CH:16]3[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]3)[C:9]=2[C:8]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][N:30]=2)=[N:7]1

Participants

4

Reactant 2

HCID 6367Acetyl chlorideHCID 136348419HCID 136348419, compound

Product 1

HCID 136348417HCID 136348417, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

Acetyl chloride (0.3 mL, 4.2 mmol) was added dropwise to methanol (20 mL), at about 0° C. Tert-butyl 4-[1-methyl-3-(2-pyridyl)-4,6,7,8-tetrahydropyrazolo[3,4-e][1,4]thiazepin-4-yl]piperidine-1-carboxylate (0.45 g, 1.1 mmol, prepared using General Procedure C from Example #2 step B with 1-Boc-piperidine-4-carboxaldehyde and thioglycolic acid followed by D) was added in portions and the resulting mixture was stirred at rt overnight. Subsequently, the mixture was concentrated in vacuo to afford 1-methyl-4-(4-piperidyl)-3-(2-pyridyl)-4,6,7,8-tetrahydropyrazolo[3,4-e][1,4]thiazepine dihydrochloride as a yellow solid which was used as such.

Workup

  1. concentrationSubsequently, the mixture was concentrated in vacuo

Sources & evidence

ORD record
ord-edc2bab988fe41a9997d5c724c8a12bb
Source dataset
uspto-grants-2015_10
Patent number
US09150592B2

Reaction notes

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